JPH05306167A - Production of short fiber reinforced c/c composite - Google Patents
Production of short fiber reinforced c/c compositeInfo
- Publication number
- JPH05306167A JPH05306167A JP4139965A JP13996592A JPH05306167A JP H05306167 A JPH05306167 A JP H05306167A JP 4139965 A JP4139965 A JP 4139965A JP 13996592 A JP13996592 A JP 13996592A JP H05306167 A JPH05306167 A JP H05306167A
- Authority
- JP
- Japan
- Prior art keywords
- composite
- fiber reinforced
- short fiber
- precursor
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、短繊維強化Ｃ／Ｃコン
ポジットの製造方法に関する。本発明の方法により得ら
れたＣ／Ｃコンポジットは、航空機やレース用車両等の
ブレーキ等に好適である。FIELD OF THE INVENTION The present invention relates to a method for producing a short fiber reinforced C / C composite. The C / C composite obtained by the method of the present invention is suitable for brakes of aircraft and racing vehicles.
【０００２】[0002]
【従来の技術】Ｃ／Ｃコンポジットは、炭素繊維強化炭
素複合材料とも称され、ＰＡＮ系、ピッチ系等の炭素繊
維の長・短繊維に、フェノール樹脂、フラン樹脂等の熱
硬化性樹脂あるいはピッチ等の熱可塑性成分を含浸又は
混合して加熱成形し、次いでこれを、非酸化性雰囲気に
おいて６００〜１，０００℃で焼成し、更に緻密化のた
めに樹脂類、ピッチ等を含浸させた後に再び焼成を繰り
返すことにより製造されている。Ｃ／Ｃコンポジット
は、前述のように、加熱、冷却を何度も繰り返して製造
されるため、その製造のために長時間を要するという問
題があった。2. Description of the Related Art C / C composites are also called carbon fiber reinforced carbon composite materials, and include long and short carbon fibers such as PAN-based and pitch-based carbon fibers, thermosetting resin such as phenol resin and furan resin, or pitch. And the like, which are then impregnated with or mixed with a thermoplastic component such as, and then heat-molded, followed by firing at 600 to 1,000 ° C. in a non-oxidizing atmosphere, and further impregnating with resins, pitch, etc. for densification. It is manufactured by repeating firing again. Since the C / C composite is manufactured by repeating heating and cooling many times as described above, there is a problem that it takes a long time to manufacture the C / C composite.
【０００３】一方、短繊維を用いたＣ／Ｃコンポジット
前駆体を製造する方法としては、例えば特開昭５４−４
１，２９５号公報には、多孔質炭素電極の製造法とし
て、ミキサーで溶媒と炭素繊維を混合した後にスクリー
ンを用いてマット化し、加圧する方法が開示されてい
る。また、特開昭６２−２５６，７６３号公報には、熱
可塑性樹脂に炭素微粉末を混合して成形した熱可塑性樹
脂シートと炭素繊維織布とを交互に積層し、樹脂の溶融
温度で加圧した後、焼成する方法が開示されている。し
かしながら、これらの方法では、嵩高い短繊維強化Ｃ／
Ｃコンポジット前駆体から緻密なＣ／Ｃコンポジットを
製造することは困難であった。On the other hand, as a method for producing a C / C composite precursor using short fibers, for example, JP-A-54-4
As a method for producing a porous carbon electrode, Japanese Patent No. 1,295 discloses a method in which a solvent and carbon fibers are mixed with a mixer and then matted using a screen, followed by pressurization. Further, in JP-A-62-256763, a thermoplastic resin sheet formed by mixing a fine carbon powder with a thermoplastic resin and molded, and a carbon fiber woven cloth are alternately laminated and heated at a melting temperature of the resin. A method of firing after pressing is disclosed. However, in these methods, bulky short fiber reinforced C /
It has been difficult to produce a dense C / C composite from a C composite precursor.
【０００４】更に、特開昭６０−５４，９７４号公報に
は、自己焼結性炭素粉末を用いて前駆体を製造し、高温
で加熱加圧処理してＣ／Ｃコンポジットを得る方法が開
示されている。しかしながら、この方法では、原料炭素
粉末の種類に制約があり、幅広い種類の炭素粉末を適用
することができないという問題があった。Further, Japanese Patent Application Laid-Open No. 60-54,974 discloses a method of producing a precursor by using a self-sintering carbon powder, and heating and pressurizing it at a high temperature to obtain a C / C composite. Has been done. However, this method has a problem that there is a limitation in the type of raw material carbon powder and a wide variety of carbon powders cannot be applied.
【０００５】[0005]
【発明が解決しようとする課題】本発明の目的は、従来
の短繊維強化Ｃ／Ｃコンポジットの製造方法よりも、容
易にかつ短時間で高密度のＣ／Ｃコンポジットを製造す
ることができる短繊維強化Ｃ／Ｃコンポジットの製造方
法を提供することにある。SUMMARY OF THE INVENTION The object of the present invention is to make it possible to produce a high density C / C composite more easily and in a shorter time than the conventional method for producing a short fiber reinforced C / C composite. It is to provide a method for producing a fiber-reinforced C / C composite.
【０００６】[0006]
【課題を解決するための手段】本発明は、短繊維状炭素
繊維及び粉砕したピッチ類を含む短繊維強化Ｃ／Ｃコン
ポジット前駆体を加圧又は拘束しながら不活性ガス雰囲
気中で４００〜１，２００℃に加熱して焼成し、得られ
た仮焼体を更に不活性ガス雰囲気中で１，５００℃以上
及び５０ｋｇ／ｃｍ2 以上の高温高圧の条件下で加熱加
圧処理する短繊維強化Ｃ／Ｃコンポジットの製造方法で
ある。According to the present invention, a short fiber reinforced C / C composite precursor containing short fibrous carbon fibers and crushed pitches is pressurized or restrained to 400 to 1 in an inert gas atmosphere. Short fiber reinforced by heating and calcining by heating to 200 ° C, and heat-pressurizing the obtained calcined body under conditions of high temperature and high pressure of 1,500 ° C and 50 kg / cm 2 or more in an inert gas atmosphere. It is a method of manufacturing a C / C composite.
【０００７】以下、本発明の内容を更に詳細に説明す
る。本発明で用いる炭素繊維は、ポリニトリルアクリル
系、ピッチ系、レーヨン系の何れであってもよく、ま
た、炭素質、黒鉛質の何れであってもよい。また、炭素
繊維は短繊維状である必要があり、通常５０ｍｍ以下、
好ましくは１〜２５ｍｍの範囲である。炭素繊維の長さ
が５０ｍｍより長くなると、この炭素繊維が成形体中に
均一に分散されず、強度が著しく低下する等の問題が生
じる。The contents of the present invention will be described in more detail below. The carbon fiber used in the present invention may be any of polynitrile acrylic type, pitch type and rayon type, and may be carbonaceous or graphitic. Further, the carbon fiber needs to be in the form of a short fiber, and is usually 50 mm or less,
It is preferably in the range of 1 to 25 mm. When the length of the carbon fibers is longer than 50 mm, the carbon fibers are not uniformly dispersed in the molded body, which causes problems such as a marked decrease in strength.
【０００８】また、Ｃ／Ｃコンポジット前駆体を形成し
た際にマトリックスとなる粉砕したピッチ類としては、
石炭系あるいは石油系の何れのピッチであってもよく、
平均粒径が１００μｍ以下、好ましくは２０μｍ以下で
あり、その軟化点が７０〜４００℃、好ましくは１５０
〜３２０℃の範囲のものが望ましく、また、該ピッチ類
は、含浸ピッチ、バインダーピッチ等の光学的に等方性
のピッチであっても、また、光学的に異方性を示すピッ
チでもよい。更に、このピッチ類については、好ましく
は炭素化収率に優れているものがよい。更に、上記ピッ
チ類には、生コークス、黒鉛粉末、カーボンブラック等
の炭素粉末を１〜５０重量％、好ましくは１〜２０重量
％の範囲で混合して使用してもよい。Further, as the crushed pitches which become a matrix when the C / C composite precursor is formed,
Any pitch of coal-based or petroleum-based,
The average particle size is 100 μm or less, preferably 20 μm or less, and the softening point is 70 to 400 ° C., preferably 150.
The pitch is preferably in the range of 320 ° C., and the pitches may be optically isotropic pitches such as impregnated pitches and binder pitches, or may be optically anisotropic pitches. .. Further, the pitches preferably have excellent carbonization yield. Further, carbon powder such as raw coke, graphite powder and carbon black may be mixed with the pitches in the range of 1 to 50% by weight, preferably 1 to 20% by weight.
【０００９】本発明方法においては、上記短繊維状の炭
素繊維と粉砕したピッチ類とから予め短繊維強化Ｃ／Ｃ
コンポジット前駆体を成形し、このＣ／Ｃコンポジット
前駆体を使用して目的とする短繊維強化Ｃ／Ｃコンポジ
ットを製造する。ここで用いる短繊維強化Ｃ／Ｃコンポ
ジット前駆体は、任意の方法で製造することができる
が、例えば、短繊維状の炭素繊維と粉砕したピッチ類と
を水等の溶媒中で均一に攪拌混合してスラリーとし、得
られたスラリーを成形用の金網型等に充填し、この金網
型の背面から真空ポンプ等で溶媒を吸引濾過し、短繊維
状の炭素繊維と粉砕したピッチ類とが均一に分散した短
繊維強化Ｃ／Ｃコンポジット前駆体を得る方法を適用す
ることができる。In the method of the present invention, short fiber reinforced C / C is previously prepared from the above short fiber carbon fibers and crushed pitches.
A composite precursor is molded, and this C / C composite precursor is used to produce an intended short fiber reinforced C / C composite. The short fiber reinforced C / C composite precursor used here can be produced by any method. For example, short fiber carbon fibers and crushed pitches are uniformly stirred and mixed in a solvent such as water. The resulting slurry is filled into a wire mesh mold for molding, etc., and the solvent is suction-filtered from the back of this wire mesh mold with a vacuum pump, etc., and the short fibrous carbon fibers and the crushed pitches are uniform. It is possible to apply a method of obtaining a short fiber reinforced C / C composite precursor dispersed in
【００１０】次に、この短繊維強化Ｃ／Ｃコンポジット
前駆体を窒素ガス等の不活性ガス雰囲気中で加圧又は拘
束下に加熱して焼成し、仮焼体とする。上記短繊維強化
Ｃ／Ｃコンポジット前駆体は、そのバックスプリング
（繊維を含む前駆体の跳ね返り）が大きく、しかも、ピ
ッチ類の溶融温度未満では結合剤となるピッチ類が溶融
しないため、加圧又は拘束を行わないと、炭素繊維とピ
ッチ類とが接着せず、この加熱焼成の過程で前駆体の形
状が損なわれ、仮焼体の製造が困難になる。この前駆体
の仮焼体を安定して成形するためにはピッチ類中の重合
成分が重合し、結合剤としての強度が発現される４００
℃以上の温度での焼成が必要である。ここで、加圧又は
拘束の手段としては、焼成温度に耐えられるものであっ
て前駆体のバックスプリングを防止できればよく、例え
ば加圧用プレス、拘束用鋼板製枠等を使用することがで
きる。Next, the short fiber reinforced C / C composite precursor is heated in an atmosphere of an inert gas such as nitrogen gas under pressure or restrained and fired to obtain a calcined body. The short fiber reinforced C / C composite precursor has a large back spring (rebound of the precursor containing fibers), and since the pitches serving as the binder do not melt below the melting temperature of the pitches, pressurization or If the binding is not performed, the carbon fibers and the pitches will not adhere to each other, and the shape of the precursor will be impaired in the process of heating and firing, making it difficult to produce a calcined body. In order to stably form the calcined body of this precursor, the polymerization components in the pitches are polymerized to develop the strength as a binder 400
Baking at a temperature of ℃ or more is required. Here, as a means for applying pressure or restraint, it is sufficient that it can withstand the firing temperature and can prevent the back spring of the precursor, and for example, a press for pressure, a steel plate frame for restraint, etc. can be used.
【００１１】また、この前駆体の焼成温度は、通常４０
０〜１，２００℃、好ましくは４００〜７００℃であ
る。この焼成温度が４００℃未満での焼成では、得られ
た仮焼体中にピッチ類由来の揮発分が多量に残存し、そ
の後工程となる高温高圧での加熱加圧処理の際に、該装
置中に揮発分を大量に導入することになり、経済的な炉
操作が困難になるという問題がある。また、この焼成は
１，２００℃以下の温度であってもピッチ類中の不純物
が充分に揮発して充分であり、焼成温度を１，２００℃
より高くしてもそれ以下の温度で焼成した場合と大差な
い。この前駆体の焼成時間は、前駆体の重量にも依存
し、通常は１〜１０時間の範囲内であり、一般には１〜
２時間で充分である。この様にして製造された仮焼体
は、その気孔率が通常約２０％以上と高く、そのままで
は実用上の嵩密度に達していない。The firing temperature of this precursor is usually 40.
The temperature is 0 to 1,200 ° C, preferably 400 to 700 ° C. When the firing temperature is lower than 400 ° C., a large amount of pitch-derived volatile components remain in the obtained calcined body, and the apparatus is used in the subsequent step of heating and pressurizing at high temperature and high pressure. Since a large amount of volatile matter is introduced therein, there is a problem that economical furnace operation becomes difficult. Further, this firing is sufficient because impurities in pitches are sufficiently volatilized even at a temperature of 1,200 ° C or lower, and the firing temperature is 1,200 ° C.
Even if it is made higher, it is not much different from the case of firing at a temperature lower than that. The firing time of this precursor also depends on the weight of the precursor and is usually in the range of 1 to 10 hours, generally 1 to
Two hours is enough. The calcined body manufactured in this manner has a high porosity of about 20% or more, and does not reach a practical bulk density as it is.
【００１２】本発明においては、この様にして得られた
仮焼体を窒素ガス等の不活性ガス雰囲気中１，５００℃
以上及び５０ｋｇ／ｃｍ2 以上、より好ましくは２，０
００〜３，０００℃及び１００〜１，０００ｋｇ／ｃｍ
2 の高温高圧の条件下で加熱加圧処理し、短時間で高密
度の短繊維強化Ｃ／Ｃコンポジットを得る。この加熱加
圧処理は、その加熱温度が１，５００℃未満であった
り、その加圧力が５０ｋｇ／ｃｍ2 未満であると、高密
度化や低気孔率化が促進されず好ましくない。この１，
５００℃以上及び５０ｋｇ／ｃｍ2 以上という高温高圧
の条件により嵩密度の向上と気孔率の低減が促進され
る。この仮焼体の加熱加圧処理における処理時間は、通
常１〜１０時間の範囲内、好ましくは１〜２時間で充分
である。例えば、２，３００℃で５００ｋｇ／ｃｍ2 と
いう高温高圧条件で１時間の加熱加圧処理を行うことに
より、嵩比重１．９０以上のＣ／Ｃコンポジットを得る
ことができる。In the present invention, the calcined body thus obtained is treated at 1,500 ° C. in an atmosphere of an inert gas such as nitrogen gas.
Or more and 50 kg / cm 2 or more, more preferably 2,0
00-3,000 ° C and 100-1,000 kg / cm
Heat and pressure treatment is performed under the conditions of high temperature and high pressure of 2 to obtain a high density short fiber reinforced C / C composite in a short time. When the heating temperature is less than 1,500 ° C. or the applied pressure is less than 50 kg / cm 2 , the heating and pressurizing treatment is not preferable because densification and low porosity are not promoted. This one
Under conditions of high temperature and high pressure of 500 ° C. or higher and 50 kg / cm 2 or higher, improvement of bulk density and reduction of porosity are promoted. The heating and pressurizing treatment time of the calcined body is usually within the range of 1 to 10 hours, preferably 1 to 2 hours. For example, a C / C composite having a bulk specific gravity of 1.90 or more can be obtained by performing heat and pressure treatment at 2,300 ° C. under a high temperature and high pressure condition of 500 kg / cm 2 for 1 hour.
【００１３】また、必要に応じて、この加熱加圧処理後
に、ピッチ類又は熱硬化性樹脂等を含浸させて再度炭化
処理することにより、より一層の嵩密度のＣ／Ｃコンポ
ジットを得ることができる。If necessary, a C / C composite having a higher bulk density can be obtained by impregnating pitches, a thermosetting resin or the like and carbonizing again after the heating and pressurizing treatment. it can.
【００１４】[0014]
【作用】上述のように、Ｃ／Ｃコンポジット前駆体を焼
成して得られた仮焼体を高温高圧条件で加熱加圧処理す
ることにより、仮焼体中の炭素繊維及び炭素間の相互拡
散が著しく促進され、炭素繊維とマトリックス炭素の接
着性が向上するものと推定され、同時に加圧によって高
密度化が促進されるものと考えられる。拡散が高密度化
に効果的であることは、仮焼体の高温高圧条件での加熱
加圧処理の際に、緻密化すること、すなわち仮焼体の厚
みが温度、圧力、保持時間に比例して収縮することから
確認でき、また、その収縮速度はアレニウス型の温度依
存性〔収縮速度＝Ｋ・ＥＸＰ（−Ｑ／ＲＴ）：但し、Ｋ
は定数を示し、Ｑは活性化エネルギーを示し、Ｒはガス
定数を示し、Ｔはホットプレス温度（絶対温度）を示
す〕を示すことからも明らかである。As described above, the calcined body obtained by firing the C / C composite precursor is subjected to heat and pressure treatment under high temperature and high pressure conditions, whereby the carbon fiber in the calcined body and the interdiffusion between carbons It is presumed that the adhesiveness between the carbon fiber and the matrix carbon is improved significantly, and at the same time, the densification is promoted by applying pressure. The fact that diffusion is effective for high density means that the calcined body is densified during heating and pressurization under high temperature and high pressure conditions, that is, the thickness of the calcined body is proportional to temperature, pressure and holding time. , And the contraction rate is dependent on the Arrhenius-type temperature dependence [contraction rate = K · EXP (−Q / RT):
Indicates a constant, Q indicates an activation energy, R indicates a gas constant, and T indicates a hot pressing temperature (absolute temperature)].
【００１５】なお、短繊維強化Ｃ／Ｃコンポジット前駆
体を直接１，５００℃以上でホットプレスすることは、
高温高圧条件下での加熱加圧処理を行う加熱加圧炉内に
ピッチ類中の揮発成分が蓄積され、このために加熱加圧
炉内の汚染が著しく、炉内の発熱体の電極部に凝集して
接地抵抗が低下するため、加熱が困難になり経済的な炉
操作ができない。また、この様な加熱加圧炉は、通常そ
の有効高さが小さいため、バックスプリングが大きな短
繊維強化Ｃ／Ｃコンポジット前駆体を当該加熱加圧炉内
に挿入するのは困難である。Hot pressing the short fiber reinforced C / C composite precursor directly at 1,500 ° C. or higher
Volatile components in the pitches are accumulated in the heating and pressurizing furnace that performs heating and pressurizing under high temperature and high pressure conditions. Since the grounding resistance is reduced due to aggregation, heating becomes difficult and economical furnace operation cannot be performed. Further, since such a heating and pressurizing furnace is usually small in effective height, it is difficult to insert the short fiber reinforced C / C composite precursor having a large back spring into the heating and pressurizing furnace.
【００１６】[0016]
【実施例】以下、実施例及び比較例に基づいて、本発明
を具体的に説明する。EXAMPLES The present invention will be specifically described below based on Examples and Comparative Examples.
【００１７】実施例１ 短繊維状炭素繊維（直径７μｍ、長さ１２ｍｍ）と粉砕
ピッチ（軟化点２４０℃、平均粒径２０μｍ）とをそれ
ぞれ重量比１：０．９の割合で水中に均一に分散してス
ラリーとし、これを金網型を用いてマット状に成形して
短繊維状炭素繊維と粉砕ピッチとが均一に分散した嵩比
重０．１の短繊維強化Ｃ／Ｃコンポジット前駆体を得
た。次に、この前駆体を大気開放型のプレスにセット
し、窒素気流中１００ｋｇ／ｃｍ2 の加圧下に、昇温速
度５０℃／分で室温から６００℃まで昇温し、そのまま
１時間保持して焼成し、仮焼体を得た。ここで、大気開
放型のプレスを用いたのは、前駆体から発生する不純物
によってプレス内部が汚染されるのを避けるためであ
る。得られた仮焼体の嵩比重は１．３０であり、また、
気孔率は３３％であった。Example 1 Short fibrous carbon fibers (diameter 7 μm, length 12 mm) and crushing pitch (softening point 240 ° C., average particle size 20 μm) were uniformly mixed in water at a weight ratio of 1: 0.9. A short fiber reinforced C / C composite precursor having a bulk specific gravity of 0.1 in which short fiber carbon fibers and crushed pitch are uniformly dispersed by dispersing the slurry into a slurry using a wire mesh mold and obtaining the slurry is obtained. It was Next, this precursor was set in a press open to the atmosphere, heated from room temperature to 600 ° C. at a temperature rising rate of 50 ° C./min under a pressure of 100 kg / cm 2 in a nitrogen stream, and kept for 1 hour. And fired to obtain a calcined body. Here, the open-air type press is used in order to prevent the inside of the press from being contaminated by impurities generated from the precursor. The bulk specific gravity of the obtained calcined body was 1.30, and
The porosity was 33%.
【００１８】更に、この様にして得られた仮焼体をホッ
トプレスにセットし、窒素気流中１００ｋｇ／ｃｍ2 の
加圧下に、昇温速度１０℃／分で室温から２，０００℃
まで昇温し、そのまま１時間保持して加熱加圧処理を行
い、Ｃ／Ｃコンポジットを作製した。前駆体の成形から
このＣ／Ｃコンポジットまでの製作に要した時間は２日
間であった。得られたＣ／Ｃコンポジットの嵩比重は
１．７０であり、また、気孔率は１５％であった。Further, the calcined body thus obtained is set in a hot press, and is heated from room temperature to 2,000 ° C. at a temperature rising rate of 10 ° C./min under a pressure of 100 kg / cm 2 in a nitrogen stream.
The temperature was raised to 1, and the temperature was maintained for 1 hour to carry out heat and pressure treatment to produce a C / C composite. The time required from the molding of the precursor to the production of this C / C composite was 2 days. The obtained C / C composite had a bulk specific gravity of 1.70 and a porosity of 15%.
【００１９】この様にして得られたＣ／Ｃコンポジット
について、更にその高密度化のため、ピッチを約１ｔｏ
ｒｒの減圧下で含浸させた後、窒素雰囲気中約１，００
０℃まで昇温して加熱し、Ｃ／Ｃコンポジットのピッチ
含浸炭化処理を行った。得られたＣ／Ｃコンポジットの
嵩比重は１．９０であり、また、気孔率は１０％であっ
た。With respect to the C / C composite thus obtained, in order to further increase the density, the pitch is set to about 1 to
After impregnation under reduced pressure of rr, about 100
The temperature was raised to 0 ° C. and heated, and the C / C composite was subjected to pitch impregnation carbonization treatment. The bulk specific gravity of the obtained C / C composite was 1.90, and the porosity was 10%.
【００２０】更に、上記ホットプレスを用いた加熱加圧
処理において、到達温度を１，５００℃、１，７５０
℃、２，０００℃及び２，３００℃と変化させ、また、
加圧力を１００ｋｇ／ｃｍ2 、３００ｋｇ／ｃｍ2 、４
００ｋｇ／ｃｍ2 及び５００ｋｇ／ｃｍ2 と変化させ、
その時の嵩比重の変化を測定した。結果は図１に示す通
りであり、この図１から高温、高圧である程その嵩密度
の向上が著しいことが判明した。Furthermore, in the heat and pressure treatment using the above hot press, the ultimate temperatures are 1,500 ° C. and 1,750.
℃, 2,000 ℃ and 2,300 ℃,
Pressurized pressure is 100 kg / cm 2 , 300 kg / cm 2 , 4
Change to 00 kg / cm 2 and 500 kg / cm 2 ,
The change in bulk specific gravity at that time was measured. The results are as shown in Fig. 1, and it was found from Fig. 1 that the bulk density was remarkably improved as the temperature and pressure were increased.
【００２１】実施例２ 実施例１で使用したと同じ前駆体を使用し、ステンレス
板でこの前駆体を厚み方向に挟み込み、ボルトとナット
で締めつけて拘束した以外は、上記実施例１と同様の焼
成条件で焼成して仮焼体を得、これを実施例１と同じ高
温高圧条件で加熱加圧処理し、更に実施例１と同様にピ
ッチ含浸炭化処理を行った。各処理工程で得られた素材
の嵩比重は、拘束焼成後の仮焼体の嵩比重が０．３０で
気孔率が著しく大であり、加熱加圧処理後のＣ／Ｃコン
ポジットの嵩比重が１．７０で気孔率が１５％であり、
ピッチ含浸炭化処理のＣ／Ｃコンポジットの嵩比重が
１．９０で気孔率が１０％であった。Example 2 The same as Example 1 except that the same precursor as that used in Example 1 was used, the precursor was sandwiched in the thickness direction by a stainless plate, and the bolt was tightened with a nut to restrain the precursor. A calcined body was obtained by firing under the firing conditions, heated and pressed under the same high-temperature and high-pressure conditions as in Example 1, and further pitch-impregnated and carbonized as in Example 1. The bulk specific gravity of the material obtained in each treatment step is 0.30 when the calcined body after binding and firing has a significantly high porosity, and the bulk specific gravity of the C / C composite after heat and pressure treatment is 1.70 and the porosity is 15%,
The pitch-impregnated carbonized C / C composite had a bulk specific gravity of 1.90 and a porosity of 10%.
【００２２】実施例３ 短繊維状炭素繊維（直径７μｍ、１２ｍｍ長さ）と粉砕
ピッチ（軟化点１５０℃、平均粒径２０μｍ）とをそれ
ぞれ重量比１：０．９の割合で水中に均一に分散してス
ラリーとし、これを金網型を用いてマット状に成形して
短繊維状炭素繊維と粉砕ピッチとが均一に分散した嵩比
重０．１の短繊維強化Ｃ／Ｃコンポジット前駆体を得
た。この様にして得られた前駆体を使用し、ステンレス
板でこの前駆体を厚み方向に挟み込み、ボルトとナット
で締めつけて拘束した以外は、上記実施例１と同様の焼
成条件で焼成して仮焼体を得、これを実施例１と同じ高
温高圧条件で加熱加圧処理し、更に実施例１と同様にピ
ッチ含浸炭化処理を行った。各処理工程で得られた素材
の嵩比重は、拘束焼成後の仮焼体の嵩比重が０．２５で
気孔率が大であり、加熱加圧処理後のＣ／Ｃコンポジッ
トの嵩比重が１．６０で気孔率が１５％であり、ピッチ
含浸炭化処理のＣ／Ｃコンポジットの嵩比重が１．８０
で気孔率が１０％であった。Example 3 Short fibrous carbon fibers (diameter 7 μm, length 12 mm) and crushing pitch (softening point 150 ° C., average particle size 20 μm) were uniformly mixed in water at a weight ratio of 1: 0.9. A short fiber reinforced C / C composite precursor having a bulk specific gravity of 0.1 in which short fiber carbon fibers and crushed pitch are uniformly dispersed by dispersing the slurry into a slurry using a wire mesh mold and obtaining the slurry is obtained. It was The precursor thus obtained was used, and the precursor was calcined under the same calcining conditions as in Example 1 except that the precursor was sandwiched in the thickness direction by a stainless steel plate, and tightened with bolts and nuts to restrain the precursor. A fired body was obtained, heated and pressed under the same high-temperature and high-pressure conditions as in Example 1, and further pitch-impregnated and carbonized in the same manner as in Example 1. Regarding the bulk specific gravity of the material obtained in each treatment step, the bulk specific gravity of the calcined body after constrained firing is 0.25, the porosity is large, and the bulk specific gravity of the C / C composite after heat and pressure treatment is 1 The porosity is 15% and the bulk specific gravity of the pitch impregnated carbonized C / C composite is 1.80.
And the porosity was 10%.
【００２３】比較例１ 比較のために、実施例１の焼成工程で得られた仮焼体を
使用し、溶融ピッチを１ｔｏｒｒの減圧下で含浸させた
後、炭化を行うピッチ含浸炭化処理を４回繰り返して行
った。この比較例１で得られた短繊維強化Ｃ／Ｃコンポ
ジットは、その嵩比重が１．６０で気孔率が２０％であ
り、製作に要した時間は約４週間であった。Comparative Example 1 For comparison, the calcined body obtained in the firing process of Example 1 was used to impregnate the molten pitch under a reduced pressure of 1 torr and then carbonize the pitch by impregnation. I went over and over again. The short fiber reinforced C / C composite obtained in Comparative Example 1 had a bulk specific gravity of 1.60 and a porosity of 20%, and the time required for production was about 4 weeks.
【００２４】上記実施例及び比較例を比較することによ
って、本発明方法により短繊維強化Ｃ／Ｃコンポジット
の製造を行うことにより、得られる短繊維強化Ｃ／Ｃコ
ンポジットの嵩密度が著しく向上するだけでなく、製作
に要する所要時間も大幅に短縮されることが判明した。By comparing the above Examples and Comparative Examples with each other, the production of short fiber reinforced C / C composites by the method of the present invention only significantly improves the bulk density of the obtained short fiber reinforced C / C composites. Not only that, it was also found that the time required for production was significantly reduced.
【００２５】[0025]
【発明の効果】本発明方法は、通常のプレスや炭化炉あ
るいはホットプレス等の加熱加圧装置を用いて、バック
スプリングの大きな短繊維強化Ｃ／Ｃコンポジット前駆
体から短時間で容易に嵩密度の高い短繊維強化Ｃ／Ｃコ
ンポジットを製造することができ、その実用的価値が高
いものである。INDUSTRIAL APPLICABILITY The method of the present invention uses a heating / pressurizing device such as an ordinary press, a carbonization furnace or a hot press to easily produce a bulk density from a short fiber reinforced C / C composite precursor having a large back spring in a short time. It is possible to produce a short fiber reinforced C / C composite having a high value, and it is of high practical value.
【図１】 図１は、ホットプレスを用いた加熱加圧処理
における加熱温度及び加圧力に対する短繊維Ｃ／Ｃコン
ポジットの嵩比重の変化を示すグラフ図である。FIG. 1 is a graph showing a change in bulk specific gravity of a short fiber C / C composite with respect to a heating temperature and a pressing force in a heating / pressing process using a hot press.
Claims (1)
を含む短繊維強化Ｃ／Ｃコンポジット前駆体を加圧又は
拘束しながら不活性ガス雰囲気中で４００〜１，２００
℃に加熱して焼成し、得られた仮焼体を更に不活性ガス
雰囲気中で１，５００℃以上及び５０ｋｇ／ｃｍ2 以上
の高温高圧の条件下で加熱加圧処理することを特徴とす
る短繊維強化Ｃ／Ｃコンポジットの製造方法。1. A short fiber reinforced C / C composite precursor containing short fibrous carbon fibers and crushed pitches is pressurized or restrained to 400 to 1,200 in an inert gas atmosphere.
It is characterized in that it is heated to ℃ and fired, and the resulting calcined body is further subjected to heat and pressure treatment in an inert gas atmosphere under conditions of high temperature and high pressure of 1,500 ° C. or higher and 50 kg / cm 2 or higher. Method for producing short fiber reinforced C / C composite.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4139965A JPH05306167A (en) | 1992-05-01 | 1992-05-01 | Production of short fiber reinforced c/c composite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4139965A JPH05306167A (en) | 1992-05-01 | 1992-05-01 | Production of short fiber reinforced c/c composite |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH05306167A true JPH05306167A (en) | 1993-11-19 |
Family
ID=15257795
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4139965A Withdrawn JPH05306167A (en) | 1992-05-01 | 1992-05-01 | Production of short fiber reinforced c/c composite |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH05306167A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR970042374A (en) * | 1995-12-30 | 1997-07-24 | 석진철 | Method for manufacturing primary carbides of carbon / carbon composites |
| JP2013511465A (en) * | 2009-11-23 | 2013-04-04 | アプライド ナノストラクチャード ソリューションズ リミテッド ライアビリティー カンパニー | CNT-infused fibers in carbon-carbon composites |
| US8999453B2 (en) | 2010-02-02 | 2015-04-07 | Applied Nanostructured Solutions, Llc | Carbon nanotube-infused fiber materials containing parallel-aligned carbon nanotubes, methods for production thereof, and composite materials derived therefrom |
| US9017854B2 (en) | 2010-08-30 | 2015-04-28 | Applied Nanostructured Solutions, Llc | Structural energy storage assemblies and methods for production thereof |
| CN107903063A (en) * | 2017-11-03 | 2018-04-13 | 大同新成新材料股份有限公司 | The method for preparing subway collector shoe sliding block using graphene metal-impregnated carbon material |
-
1992
- 1992-05-01 JP JP4139965A patent/JPH05306167A/en not_active Withdrawn
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR970042374A (en) * | 1995-12-30 | 1997-07-24 | 석진철 | Method for manufacturing primary carbides of carbon / carbon composites |
| JP2013511465A (en) * | 2009-11-23 | 2013-04-04 | アプライド ナノストラクチャード ソリューションズ リミテッド ライアビリティー カンパニー | CNT-infused fibers in carbon-carbon composites |
| US8999453B2 (en) | 2010-02-02 | 2015-04-07 | Applied Nanostructured Solutions, Llc | Carbon nanotube-infused fiber materials containing parallel-aligned carbon nanotubes, methods for production thereof, and composite materials derived therefrom |
| US9017854B2 (en) | 2010-08-30 | 2015-04-28 | Applied Nanostructured Solutions, Llc | Structural energy storage assemblies and methods for production thereof |
| US9907174B2 (en) | 2010-08-30 | 2018-02-27 | Applied Nanostructured Solutions, Llc | Structural energy storage assemblies and methods for production thereof |
| CN107903063A (en) * | 2017-11-03 | 2018-04-13 | 大同新成新材料股份有限公司 | The method for preparing subway collector shoe sliding block using graphene metal-impregnated carbon material |
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